headspace solid phase microextraction (HS-SPME)

Top PDF headspace solid phase microextraction (HS-SPME):

Headspace analysis of natural yoghurt using headspace solid phase microextraction : a thesis presented in partial fulfilment of the requirements for the degree of Master of Philosophy in Food Technology at Massey University (Turitea Campus), Palmerston No

Headspace analysis of natural yoghurt using headspace solid phase microextraction : a thesis presented in partial fulfilment of the requirements for the degree of Master of Philosophy in Food Technology at Massey University (Turitea Campus), Palmerston North, New Zealand

The main objective of this study was to devise a methodology for the Headspace Solid Phase Microextraction HS-SPME technique to investigate and quantify six flavour analytes in natural, [r]

26 Read more

Simultaneous Determination of Disinfection By-products in Water Samples from Advanced Membrane Treatments by Headspace Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry

Simultaneous Determination of Disinfection By-products in Water Samples from Advanced Membrane Treatments by Headspace Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry

A headspace-solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) method has been developed for the simultaneously determination of 20 disinfection by-products (DBPs) in water samples from reverse osmosis (RO) membranes. Selected compounds belong to different families including: trihalomethanes (THMs), halogenated acetonitriles (HANs), halogenated nitromethanes (HNMs), halogenated ketones (HKs) and other halogenated DBPs. Four commercial fibres with different polarities were tested for the extraction of the compounds and the main variables affecting HS-SPME such as extraction time, extraction temperature and pH of the samples were optimized by applying a central composite design.
Show more

12 Read more

Optimization of headspace solid-phase microextraction conditions for the identification of volatiles compounds from the whole fruit of lemon, lime, mandarin and orange

Optimization of headspace solid-phase microextraction conditions for the identification of volatiles compounds from the whole fruit of lemon, lime, mandarin and orange

excessively used for the analysis of volatile compounds. The HS-SPME technique is a new, simple, rapid, eco-friendly and solvent-free sample preparation tech- nique for the extraction of volatile compounds [16] [17]. The HS-SPME tech- nique gives simultaneously tens or hundreds of possible volatile compounds and also provides interesting results when gas chromatography (GC) is combined with either Flame Ionization Detector (FID) or mass spectrometric detection (MS), but it must be optimized for the volatiles being targeted [18] [19]. Many factors can affect the optimization of extraction conditions, such as the correct fibre and an appropriate chamber for capturing the VOCs, the temperature used during extraction and the extraction time from the headspace [20]. So far, there has been no systematic work on optimizing extraction conditions for whole fresh citrus fruit. Therefore, this study will determine the optimal conditions of seal- ing time, extraction time and chamber size for citrus fruit volatile isolation by the headspace solid phase microextraction (HS-SPME) technique with gas chromatography coupled with Flame Ionization Detector GC-FID.
Show more

11 Read more

Analysis of aroma components of dark teas from five different production regions by fully automatic headspace solid phase microextraction coupled with gas chromatography mass spectrometry

Analysis of aroma components of dark teas from five different production regions by fully automatic headspace solid phase microextraction coupled with gas chromatography mass spectrometry

With the aim to study the volatile aroma component of dark teas from five different production regions (Yunnan, Hunan, Sichuan, Guangxi, and Hubei) in China, the fully automatic headspace solid-phase microextraction (HS-SPME) method was constructed for extracting the volatiles and gas chromatography-mass spectrometry (GC-MS) coupled with retention index (RI) of the volatiles were used to determine the volatiles variety in dark tea samples. The result showed that 105 aroma constituents were determined in five dark teas, mainly including alcohols, ketones, hydrocarbons, and methoxy-phenolic compounds, etc. Among which the methoxy-phenolic compounds were the most abundant components in the Pu-erh ripe tea, mainly including 1,2,3-trimethoxybenzene, 1,2,3-trimethoxy-5-methylbenzene, and 1,2,4-trimethoxy benzene. Ketones were the most abundant components in the Heimao tea and Yaan dark tea, mainly including β-ionone, geranyl acetone, and 6,10,14-trimethyl-2-pentadecanone. While the hydrocarbons were the most abundant components in the Liubao tea and Qingzhuan tea, mainly including 2,6,10,14-tetramethyl-pentadecane, 2,6,10,14-tetramethyl-hexadecane, and heptadecane, etc. In comparison, there were remarkable differences in flavor and aroma composition of the five types of dark tea, which may be related to the different species or subspecies, growing region and processing technology.
Show more

8 Read more

Characterization of volatile compounds of Daucus crinitusDesf. Headspace Solid Phase Microextraction as alternative technique to Hydrodistillation

Characterization of volatile compounds of Daucus crinitusDesf. Headspace Solid Phase Microextraction as alternative technique to Hydrodistillation

The essential oils of aromatic herbs are traditionally obtained using hydrodistillation. Because the emitted volatile fraction plays a fundamental role in a plant’s life, various novel techniques have been developed for its extraction from plants. Among these, headspace solid phase microextraction (HS-SPME) allows for the rapid fingerprinting of a plant’s headspace [7-10], and HS sampling requires the optimization of the extraction parameters to be carried out. As has been previously reported in the literature [9,10], the most effective fibers from vegetable matrices used are those consisting of three polymers: a liquid (PDMS) for the less polar com- ponents, and two solids, DVB and CAR, for the more polar components. Several conditions regarding the time and temperature for equilibrium and extraction have been reported, according the plant material analyzed [7-10].
Show more

15 Read more

Optimization of the Headspace Solid-Phase Microextraction Gas Chromatography for Volatile Compounds Determination in
Phytophthora Cinnamomi Rands

Optimization of the Headspace Solid-Phase Microextraction Gas Chromatography for Volatile Compounds Determination in Phytophthora Cinnamomi Rands

Abstract— Phytophthora cinnamomi (P. c) is a plant pathogenic oomycete that is capable of damaging plants in commercial production systems and natural ecosystems worldwide. The most common methods for the detection and diagnosis of P. c infection are expensive, elaborate and time consuming. This study was carried out to examine whether species specific and life cycle specific volatile organic compounds (VOCs) can be absorbed by solid-phase microextraction fibers and detected by gas chromatography that are produced by P. c and another oomycete Pythium dissotocum. A headspace solid-phase microextraction (HS-SPME) together with gas chromatography (GC) method was developed and optimized for the identification of the VOCs released by P. c. The optimized parameters included type of fiber, exposure time, desorption temperature and desorption time. Optimization was achieved with the analytes of P. c+V8A and V8A alone. To perform the HS-SPME, six types of fiber were assayed and compared: 7μm Polydimethylsiloxane (PDMS), 100μm Polydimethylsiloxane (PDMS), 50/30μm Divinylbenzene/Carboxen TM /Polydimethylsiloxane
Show more

5 Read more

Nuclear Magnetic Resonance and Headspace Solid-Phase Microextraction Gas Chromatography as Complementary Methods for the Analysis of Beer Samples

Nuclear Magnetic Resonance and Headspace Solid-Phase Microextraction Gas Chromatography as Complementary Methods for the Analysis of Beer Samples

Abstract: Chemical analysis of the organic components in beers has applications to quality control, authenticity and improvements to the flavor characteristics and brewing process. This study aims to show the complementary nature of two instrumental techniques which in combination can identify and quantify the majority of organic components in a beer sample. Nuclear Magnetic Resonance (NMR) was used to provide concentrations of twenty five different organic compounds including alcohols, organic acids, carbohydrates, and amino acids. Calorie content was also estimated for the samples. NMR data for ethanol concentrations were validated by comparison to a Fourier Transform Infrared Spectrometry (FTIR) method. Headspace Solid-Phase Microextraction (SPME) Gas Chromatography Mass Spectrometry (GCMS) was used to identify a range of volatile compounds such as alcohols, esters and hop derived aroma compounds. A simple and inexpensive conversion of a Gas Chromatography Flame Ionization Detector (GC FID) instrument to allow the use of Solid-Phase Microextraction was found to be useful for the quantification of volatile esters.
Show more

12 Read more

Headspace analysis of natural yoghurt using headspace solid phase microextraction : a thesis presented in partial fulfilment of the requirements for the degree of Master of Philosophy in Food Technology at Massey University (Turitea Campus), Palmerston No

Headspace analysis of natural yoghurt using headspace solid phase microextraction : a thesis presented in partial fulfilment of the requirements for the degree of Master of Philosophy in Food Technology at Massey University (Turitea Campus), Palmerston North, New Zealand

The results suggested that the two methods were complementary in that the SH method extracted the more volatile compounds acetaldehyde, acetone and 2-butanone whereas, the HS-SPME method[r]

260 Read more

Integration of GC MS Based Non Targeted Metabolic Profiling with Headspace Solid Phase Microextraction Enhances the Understanding of Volatile Differentiation in Tobacco Leaves from North Carolina, India and Brazil

Integration of GC MS Based Non Targeted Metabolic Profiling with Headspace Solid Phase Microextraction Enhances the Understanding of Volatile Differentiation in Tobacco Leaves from North Carolina, India and Brazil

In this report, gas chromatography-mass spectrometry (GC-MS) based non-targeted metabolomics is used to develop appropriate headspace solid phase microextractions (HS-SPME) to enhance the understanding of volatile complexity of flue-cured tobacco leaves. Non-targeted metabolic profiling of GC-MS shows that the extraction condition of HS- SPME at 100˚C for 30 min provides a better metabolite profile than other extraction conditions tested. GC-MS and principal component analyses (PCA) show that among five types of fibers tested, 100 μm polydimethylsiloxane (PMDS), 65 μm polydimethylsiloxane/divinylbenzene (PMDS/DVB) and 75 μm carboxen/polydimethylsiloxane (CAR/ PMS) provide a better reproducible metabolite profile. Based on an appropriate PDMS extraction condition optimized, we use GC-MS analysis and PCA to compare metabolite profiles in flue-cured leaves of tobacco plants grown in North Carolina, India and Brazil, respectively. The resulting data of PCA show that the global metabolic profiles in North Carolina samples are separated from those in Brazil and India samples, two groups of which are characterized by a par- tially overlapped pattern. Several peaks that were differentially accumulated in samples were annotated to known me- tabolites by deconvolution analysis, such as norsolanadione, solavetivone and rishitin. Norsolanadione is detected only in Brazil samples. Solavetivone is detected in samples of India and Brazil but not in those of North Carolina. Rishitin is detected in samples of North Carolina and India but not in Brazil samples. These data indicate that not only can a non-targeted metabolic profiling approach enhance the understanding of volatile complexity, but also can identify marker volatile metabolites in tobacco leaves produced in different growth regions.
Show more

11 Read more

Application of Polypyrrole Coated Stainless-Steel Wire to the Headspace Solid-Phase Microextraction of Aliphatic Amines

Application of Polypyrrole Coated Stainless-Steel Wire to the Headspace Solid-Phase Microextraction of Aliphatic Amines

The analytical performance characteristics of the headspace SPME procedure, under optimum conditions, were evaluated and are shown in Table 1. To determine the repeatability, seven replicate experiments were carried out by extracting a spiked water sample (500.0 µg.L −1 ) of each compound. The relative standard deviations (RSDs) were between 3.6 and 4.3%. The linearity of the method was tested using target aliphatic amines in the concentration range of 90-1600 µg.L −1 . For each level, three replicate extractions and determinations were performed. This method showed a good linear behavior in the tested range, with correlation coefficients ranging between 0.981 and 0.991. The enrichment factor, defined as the ratio of peak heights after extraction and that before extraction [28], was calculated using the average of the three trials obtained for 500.0 µg.L −1 concentration level. The enrichment factors of the proposed method ranged from 170 to 234. Limits of detection (LODs) calculated as three times the baseline noise, were in the range of 0.9- 1.6 µg.L −1 (Table 1).
Show more

7 Read more

The Essential Oils from Pittosporum tobira Flowers Display Antiproliferative Properties and Inducing Apoptosis on Lung Carcinoma Cells

The Essential Oils from Pittosporum tobira Flowers Display Antiproliferative Properties and Inducing Apoptosis on Lung Carcinoma Cells

Background: Pittosporum tobira (Thunb.) Aiton is an aromatic medicinal plant widely cultivated in the world. However, the essential oils (EOs) from P. tobira flowers for anti-cancer potential is still not systematically studied. The present aim to elucidate the phytochemical composition of the EOs and to explore mechanism of anticancer action. Methods: The EOs were extracted and analyzed by headspace solid-phase microextraction (HS-SPME) with gas chromatography-mass spectrometry (GC-MS). Volatile components were identified according to Kovats retention index (KI) and NIST database. The anti-neoplasm mechanisms of the EOs was comprehensively investigated in lung carcinoma A549 and H460 cells. Results: A total of 47 secondary metabolites representing 94.18% of the EOs were successfully identified: monoterpenes and sesquiterpenes were the dominant terpenoids. The EOs exhibited antiproliferative activity on A549 and H460 lung carcinoma cells. Hoechst 33324 fluorescent staining indicated the typical characteristics of apoptosis and induced cycle phase arrest. AnnexinV/PI staining revealed that the number of apoptotic cells was increased. Furthermore, the EOs also induced the caspase-mediated mitochondrial apoptosis pathway. Conclusions: Findings suggest that the full-scale chemical composition and first characterization of anticancer activities of the EOs, it could be used for integrative natural anti-cancer agents in health care should be pay more attention.
Show more

10 Read more

Chemical Analysis of Volatile Constituents of Pulicaria Mauritanica Isolated by Hydrodistillation and Headspace Solid-phase Micro-extraction Techniques. Antimicrobial Activity of its Essential Oil

Chemical Analysis of Volatile Constituents of Pulicaria Mauritanica Isolated by Hydrodistillation and Headspace Solid-phase Micro-extraction Techniques. Antimicrobial Activity of its Essential Oil

There are various techniques available for extracting volatile components from aromatic plants. Hydrodistillation (HD) is a conventional method used to extract EOs, because it can be easily implemented in industry and has no chemical pollution. However, it has certain disadvantages, particularly, the consumption of energy and time, the deterioration of heat-sensitive compounds and the low extraction yields of EOs. Thus, developing an alternative rapid, sensitive, safe, and energy-conserving extraction technique is highly desirable. Thereby, headspace solid- phase microextraction (HS-SPME) is an easy, fast and modern sample preparation technique to characterize the volatile fraction (VF) of aromatic and medicinal plants [7]. Pulicaria, established in 1791 by Gaertner, is a genus of flowering plant of the Asteraceae family, containing more than 77 species available in the world 8. P. mauritanica Coss. is an aromatic and endemic plant growing wild in Southeast of Morocco. It is an herb branched, woolly-rooted perennial and creeping; its leaves are less broad, oval- lanceolate, endowed with a very strong odor; the flowers are yellow where it blooms in March-May. The plant abounds woodlands, rockeries on dry rocky pastures and in the plains and low mountains up to 1500 m (Fig. 1). This Moroccan medicinal plant, locally known as “Ifanzi oudaden”, is endowed with a very strong and very pleasant smell making it usable as a flavoring of tea and as an ingredient for perfuming baths. It is also used in traditional local medicine thanks to these antispasmodic properties, hyperglycemic and repellent properties against insects [9] and in the treatment of dysentery [10,11.
Show more

13 Read more

Determination of volatile alkylpyrazines in microbial samples using gas chromatography-mass spectrometry coupled with head space-solid phase microextraction

Determination of volatile alkylpyrazines in microbial samples using gas chromatography-mass spectrometry coupled with head space-solid phase microextraction

flavors according to the nature of the alkyl substituents. Therefore, the understanding synthesized pyrazines from microbial metabolism for finding key flavors is very im- portant. However, analysis of pyrazines in food has been investigated actively, while few studies have been per- formed in analytical methods of pyrazines from micro- bial metabolism. Furthermore, pyrazines produced by microorganisms can be found in low quantities in cul- ture media (Beck et al. 2003; Dickschat et al. 2010; Nawrath et al. 2010), and the bottleneck of analysis has been the difficulty of sample preparation due to the high solubility and volatility of pyrazines in microbial sam- ples. Conventional techniques have been used previously such as headspace and purge and trap. Headspace ex- traction used for volatile analytes in solid or liquid sam- ples is preferable technique for a quality control but the sensitivity is limited (Pawliszyn 2000). The purge and trap technique is more sensitive, while the complicated switching valves and ghost peaks caused by decompos- ition of the trapping materials during thermal desorption are main disadvantages. Recently, SPME which was invented by Pawliszyn in 1989 has been applied to ana- lysis in various fields, such as environmental chemistry, forensic chemistry, pharmaceutical, food, beverage, and flavors (Pawliszyn 2000; Theodoridis et al. 2000). The advantages of SPME over the previous techniques are that it is a very simple and efficient sample preparation method as sampling, extraction, and concentration can be combined into a single solvent-free step. Other ad- vantages of SPME are that it can use small sample vol- umes (Risticevic et al. 2010). As a diffusion micro sampling tool, solid porous coating fibers can adsorb analytes from a sample by immersion or headspace ex- traction. Generally, direct immersion is not suitable for complex media and may damage fiber in direct contact with dirty matrix (Pawliszyn 2000). For these reasons, headspace-solid phase microextraction (HS-SPME) was adopted to determine volatile alkylpyrazines (VAPs) in microbial samples as a sampling technique in this study. Meanwhile, the nitrogen–phosphorus detector (NPD) or
Show more

8 Read more

Optimized Method to Analyze Rose Plant Volatile Organic Compounds by HS SPME GC FID/MSD

Optimized Method to Analyze Rose Plant Volatile Organic Compounds by HS SPME GC FID/MSD

A method involving Headspace solid-phase microextraction (HS-SPME) fiber combined with gas chromatography (GC) coupled with flame ionization de- tection (FID) and gas chromatography with mass spectrometry (GC-MS) was developed and optimized to investigate volatile organic compounds (VOCs) from different tissues (flowers, leaves, stems, rhizosphere and whole plants) of Floribunda and Hybrid Tea roses (intact and cut). Three-phase fiber 50/30 µm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) was used. Two types of chambers (Tedlar bag and glass jar) were evaluated for collection of VOCs and glass jar was selected. Absorbed compounds on the fiber were completely desorbed in the GC injector port at three desorption times (5, 10 and 15 min), and 5 min at 250˚C was used. The maximum extraction effi- ciency for flowers tissues (equilibrium absorption) was achieved 2 h after fiber exposure in the headspace for intact and cut Floribunda and Hybrid Tea flowers. Under the optimized HS-SPME and GC-FID/MS conditions, 1h ex- traction time was chosen for intact and cut Floribunda and Hybrid Tea leaves and stems. The results demonstrated that 5 cm depth was selected for root and soil part (rhizosphere) for both rose cultivars, and 6 h and 12 h extraction time of VOCs from rhizosphere was achieved for Floribunda and Hybrid Tea, respectively. One hour was chosen for VOCs released from whole rose plants for both cultivars. In this study, the VOC profiles of two rose cultivars were characterized by the optimized HS-SPME-GC method. The different tissues of rose plants gave wide range of the VOCs; also the chromatograms of different cultivars were quite different and the specific VOC pattern of rose types de- pends on the species. Results from this study demonstrate the feasibility of this method for identifying VOCs from two rose cultivars and the potential use of this method for physiological studies on rose plants or on other flori- culture plants.
Show more

19 Read more

Quantitative Monitoring of the Volatiles from The Aerial Parts of Satureja Hortensis by The Use of HS-SPME-GC-MS Approach

Quantitative Monitoring of the Volatiles from The Aerial Parts of Satureja Hortensis by The Use of HS-SPME-GC-MS Approach

The volatile fractions isolated from the ground aerial parts of Satureja hortensis were trapped using the headspace solid phase microextraction (HS-SPME) strategy and subsequently monitored using gas chromatography in combination with mass spectrometry (GC-MS) instrumentation. Eleven constituents were totally recognized in the analyzed volatile parts, representing entire of the corresponding profile. Among the natural groups present in the chemical profile, monoterpene hydrocarbons (99.5%) were found as the major constituents with the dominant compounds being γ-terpinene (46.0%), p-cymene (11.8%), α-terpinene (11.1%), α-pinene (10.4%) and α-thujene (6.8%). However, lower contents of some natural compounds including myrcene (5.2%), β-pinene (3.9%), o-cymene (2.6%), α-phellandrene (1.1%), camphene (0.6%) and thymol (0.5%) were identified. Accordingly, only 0.5% of the profile included oxygenated monoterpenes.
Show more

8 Read more

Liquid and solid phase microextraction methods for the analysis of organic environmental pollutants

Liquid and solid phase microextraction methods for the analysis of organic environmental pollutants

Aguinaga, N., Campillo, N., Vinas, P., and Hernandez-Cordoba, M. (2008). A Headspace Solid-Phase Microextraction Procedure Coupled with Gas Chromatography-Mass Spectrometry for the Analysis of Volatile Polycyclic Aromatic Hydrocarbons in Milk Samples. Anal. Bioanal. Chem. 391, 753-758. Alcudia-Leon, M.C., Lucena, R., Cardenas, S., and Valcarcel, M. (2011a). Stir

45 Read more

Volatile composition analysis by solid-phase microextraction applied to oak wood used in cooperage (Quercus pyrenaica and Quercus petraea): effect of botanical species and toasting process

Volatile composition analysis by solid-phase microextraction applied to oak wood used in cooperage (Quercus pyrenaica and Quercus petraea): effect of botanical species and toasting process

Before the first daily analysis, the fiber was conditioned for 5 min at 250°C in the gas chromatograph (GC) injector. An aliquot of 10 ml of model wine solution or 1 g of oak wood-chip sample was transferred into a 22-ml vial and the aroma compounds were extracted by headspace SPME for 30 min at 25°C. Prior to extraction, 3 g of NaCl (at saturation level) was added to each sample of the model wine solution. This was because maximum extraction is obtained from salt-saturated samples using NaCl. 39

8 Read more

Developments/Application of Ionic Liquids/Poly Ionic Liquids in Magnetic Solid-Phase Extraction and Solid Phase Microextraction

Developments/Application of Ionic Liquids/Poly Ionic Liquids in Magnetic Solid-Phase Extraction and Solid Phase Microextraction

Many studies aimed to exploit the hydrogen bond accepting property of the chloride anion so as to extract polar analytes including phenols, volatile fatty acids (VFAs), and alcohols. For comparison purposes, a PIL containing the same cation but paired with bis [(trifluoromethyl) sulfonyl] imide anion, known to possess significantly low hydrogen bond basicity, was also used to extract the same analytes. In addition to performing the extraction in an aqueous matrix, heptane was also employed as the extraction solvent to investigate the selectivity of the PIL coatings towards different analytes using headspace extraction [75].
Show more

9 Read more

Determination of some selected pesticide residues in apple juice by solid-phase microextraction coupled to gas chromatography – mass spectrometry

Determination of some selected pesticide residues in apple juice by solid-phase microextraction coupled to gas chromatography – mass spectrometry

sampled with PA (85  m) and PDMS (100  m) fi bres. The fi bre coating was directly exposed to the aque- ous phase at room temperature. Due to the rather low vapour pressures and volatilities of the target pesticides headspace sampling would not be so suc- cessful. Both fi bre coatings showed suffi cient extrac- tion yields to reach the trace concentration needed for the detection in apples and derived juice (Fig. 1). Finally, the PDMS fi bre was preferred for the analy- ses in this work due to its robustness and known ab- sorption phenomena those can be related to phys- ico-chemical properties of the analytes and allows some mechanistical interpretation of data.
Show more

8 Read more

Solid phase microextraction analysis of volatile constituents of heated palm olein and selected oils

Solid phase microextraction analysis of volatile constituents of heated palm olein and selected oils

The oil sample (5 g) was subjected to accelerated oxidation by heating at 40°, 60°, 80°, 100°, 120°, 140°, 160° and 180°C in a 15-ml open vial. The internal standard solution, i.e. n-dodecane (5 µg/g) was injected into the headspace vial for the pur pose of quantification of the volatile constituent. After heating the sample for 30 min., the volatiles from the oil were collected using a SPME headspace sampling system as previously described 13 . The PDMS fibre was placed in the

8 Read more

Show all 10000 documents...